The purpose of this paper is to invent a new functional coated fabric based on nanomaterials to shield UV and IR. Multifunctional surface coatings with ultraviolet (UV)/near infrared radiations protection and waterproof were widely applied in outdoor fabrics. Herein, ultrafine TiO2 and nano-antimony doped tin dioxide (ATO) were prepared and embedded into water-based polyurethane (PU) coatings and then coated on the nylon fabric.
ATO was prepared using the sol–gel method and the two powders were dispersed by ball milling. The results of zeta potential and particle size distribution showed that the ultrafine TiO2 and nano-ATO could be stably dispersed in water at pH 8 with the presence of sodium polycarboxylate. The optimal process was screened out by orthogonal design and scanning electron microscopy (SEM), UV protection, thermal insulation and water-pressure resistance were tested. SEM images indicated the nanoparticles could be uniformly dispersed in the coatings.
The effect of UV prevention can get to UPF > 50, UVA < 5 per cent, which meet up with the AATCC 183-2014. Coatings can effectively lower the temperature of fabric surface by 8∼9ºC through the self-made closed test system and by 3ºC through the open test system.
These PU coatings are environment-friendly and adhesive to impart waterproof, UV-proof and thermal insulation properties to nylon fabrics by coating finishing.
Zhang, W., Yao, J. and Wang, S. (2019), "Multifunctional outdoor fabrics with ATO and TiO2 embedded PU coatings", Pigment & Resin Technology, Vol. 48 No. 4, pp. 348-356. https://doi.org/10.1108/PRT-08-2018-0087
Emerald Publishing Limited
Copyright © 2019, Emerald Publishing Limited
Recently, the need for smart multifunctional textiles are increased for comfortable and safety properties to the end users. There are several important functions have to be inserted in textile fibers such as ultraviolet (UV) protection (Shaheen et al., 2016), flame retardancy (Grancaric et al., 2017; Zhang et al., 2016), hydrophobicity (Jeyasubramanian et al., 2016; Przybylak et al., 2016), thermal insulation (Lu et al., 2017) and antibacterial properties (Heliopoulos et al., 2013). The UV protection is one of the important properties for outdoor fabrics. The UV spectrum has three groups based on wavelength, namely, UVC consists of wavelength from 100 to 290 nm, UVB (290∼320 nm) and UVA (320∼400 nm) (Velasco et al., 2008). The UV radiation coming from sunlight can create several negative health effects such as acceleration of skin damage and aging, photodermatosis, erythema and even mild-to-sever skin cancer (Shaheen et al., 2016), ZnO and TiO2 were widely used as UV-protected materials on textile. They are n-type semiconductor materials with band-gap energy 3.37 eV of ZnO and 3.2 eV of TiO2 (Ke et al., 2017; Wang et al., 2016). ZnO and TiO2 are regarded as candidates for sun blockers for the UV radiation due to their sensitivity to the UV radiation (Inamdar and Rajpure, 2014; Li et al., 2014a).
In the past decades, thermal insulation materials were widely applied in textiles and buildings to keep the human warm and dry in cold climates and protect them from the heat and sun in warm climates (Schuster et al., 2006). As the environmental conditions change, thermo physiological comfort is an important aspect of apparel, and relevant attributes of garments become even more important inactive sportswear (Watson et al., 2013; Ho et al., 2008; Rengasamy et al., 2009). Transparent conducting oxides are important materials in the field of thermal insulation. The n-type semiconductors, such as indium tin oxide (ITO), antimony doped tin dioxide (ATO) and aluminum doped zinc oxide (Goebbert et al., 1999), are widely used as thermal insulation materials in these applications (Mei et al., 2012; Wang et al., 2010). Among these semiconductors, ATO is a well-known material with super optical, electrical properties, infrared light insulation, good stability and relatively low cost, which has attracted attention as a promising material in environment protection and energy conservation (An et al., 2016; Zhong et al., 2012). ATO nanoparticles can be used to prepare thermal insulation glass paint for its high transmittance in visible light and effective infrared shielding performance at the same time (Li et al., 2014c; Tan et al., 2014).
Polyamide fiber is an important and abundantly used fabric in both military and civilian areas due to the low cost, good abrasion resistance, etc (Liu et al., 2010; Kundu et al., 2018). However, its flammability and anti-ultraviolet properties to be improved also limit its further applications (Zhao et al., 2014; Liang et al., 2000). In this work, multi-functional polyurethane (PU) coatings embedding nano-ATO and TiO2 on textiles would be prepared. These coatings would have UV protection, thermal insulation and waterproof properties. To this end, the synthesized nano-ATO and TiO2 suspensions mixed with PU emulsions were prepared and then coating on a piece of nylon fabric. The multi-functional nylon fabric would be created after drying. The anti-UV, thermal performance, waterproof and mechanical properties of nylon fabric with PU coatings were investigated.
The 210T colorless nylon (62 g/m2) with 25 × 20 cm were used as the substrates; 2,024 aluminum, specifications: 30 × 20 × 1 mm, black; 500 mL PU ball milling tank; stannic chloride pentahydrate; antimony trichloride; sodium hydroxide; aqueous ammonia; and hydrochloric acid were all analytical reagent grade and purchased from Sinopharm Chemical Reagent Group Co. Ltd. (Shanghai, China). Polycarboxylate, ultrafine TiO2 powder, water-based PU coating adhesive, thickener DM-5239, waterproofing agent AG-E081, dispersant 5,040 were all industrial reagent grade and purchased from Nopco Co., Ltd.
Preparation of nano-antimony doped tin dioxide dispersion
The 0.45 mol/L of SnCl4•5H2O ethanol solution and 0.05 mol/L of SbCl3 ethanol solution were mixed and thoroughly stirred for 1 h. Another 25-28 per cent (mass fraction) aqueous ammonia solution was prepared and slowly added to the above solution by drop till the pH of the solution was 7. The synthesized ATO precursor sol was separated by centrifugation, washed with distilled water several times, and then dried to a powder at 100°C. It was placed in a crucible and heated at 800°C for 1 h in a muffle furnace to obtain a nano-ATO blue powder (Li et al., 2014b).
The amount of 6 g of nano-ATO was dispersed in 200 mL of water, 3 drops of dispersant 5,040 were added, ultrasonically dispersed, ball milled for 6 h, and zirconium beads were 0.8 mm in size to obtain a blue nano-ATO dispersion.
Waterproof finishing of fabric
The waterproof agent AG-E081 was dissolved in 100 mL water firstly. The nylon (25 × 20 cm) was introduced into the finishing bath by double-dip double-nip method at room temperature, followed by pre-baked at 110°C for 1.5 min and baked at 170°C for 1 min.
General coating finishing
The water-based coating adhesive was diluted in water, added 1.2 g thickener DM-5239, stirred and prepared into 100 g coating finish agent. Then the agent was coated on the nylon fabric. Two layers were coated on the fabric and each layer amount of 30 g ± 2 g/m2, and then dried in the oven at 60°C.
Functional coating finishing
A certain amount of the nano-dispersion was diluted in water, coating adhesive and thickener were added and stirred uniformly to prepare 100 g finishing agent. Then it was applied to the waterproof finished fabric by coating. Two layers were coated on the fabric and each layer amount of 30 g ± 2 g/m2, followed by drying in the oven at 60°C. The performances of water-pressure resistance, anti-UV and thermal insulation were tested.
Instruments and characterization
The particle size and distribution of nano-materials were determined by nano-zs laser particle size analyzer (Malvern, Britain). Scanning electron microscopy (SEM) was used to observe the distribution, size and uniformity of the nanoparticles and the coated gel on the fabric surface (Hitachi, Japan). UV-1000 F transmittance tester was used to measure the anti-UV effect of the fabric, and the UV transmittance and UPF were measured according to the AATCC 183-2010 with Evaluation of the anti-UV properties of textile (Labsphere, USA). The infrared transmittance, reflectance and absorptivity of the fabric were measured by UV-4100 UV-Vis-NIR spectrophotometer. A simulated thermal shielding test was conducted using a self-made thermal insulation box with the top covered with the coated textile and irradiated by an iodine tungsten lamp with 500 W. The temperature varying on the bottom covered with black aluminium plate was tested by a thermocouple logger. Fabrics were tested and evaluated according to AATCC 22-2005 Spray test method (Shanghai, China). The water-pressure resistance test was carried out according to AATCC 127-2013.
Results and discussion
The ultrafine TiO2 powder was selected as the main anti-UV material and the auxiliary insulating materials and nano-ATO was the main thermal insulation.
The X-ray diffraction (XRD) pattern of the nano-ATO powder was shown in Figure 1(a). It can be seen that the XRD data of the obtained ATO composite powder sample corresponded to the Joint Committee on Powder Diffraction Standards spectrum (21-1,250) data of the tetragonal phase SnO2, indicating that the ATO powder sample has a tetragonal phase rutile structure after calcination at 800°C for 1 h. There was no diffraction peak of Sb or other impurities in the sample and indicated the doping Sb did not form a new phase structure, and the doping atom Sb only replaced the position of Sn in the crystal lattice. Due to the difference in the ionic radius of Sb3+, Sb5+ and Sn4+, and the grain size was small, the defects on the surface and interface were infiltrated into the interior, causing the lattice to be distorted and the XRD peak shift. Figure 1(b) showed that the average particle size of nano-ATO dispersion after ball milling was 527 nm.
Effect of pH on zeta potential of dispersion
According to the electric double layer model of the DLVO theory, the surface of the dispersed particles is charged, and the surface charge of the particles is increased by adjusting the pH of the solution or by adding an electrolyte to form an electric double layer. The zeta potential increases and electrostatic repulsion occurs between the particles. When the absolute value of the zeta potential of the particle is the largest, the electric double layer of the particles exhibits the maximum repulsive force to disperse the particles; when the zeta potential of the particle is equal to zero, the attraction between the particles is greater than the repulsive force between the electric double layer, and the particles agglomerates and settles. Zeta potential of ATO dispersions with different pH values was shown in Figure 2(a). The isoelectric point of the nano-ATO particles was between pH 1-2. When the pH was less than the isoelectric point, the nanoparticles were positively charged and the pH was greater than the isoelectric point, the nanoparticles were negatively charged. At more than pH 5, the absolute value of the zeta potential of the dispersion was greater than 40 mV. The absolute value of zeta potential reached the maximum at pH 8, where the dispersion was most stable. The zeta potential of ultrafine TiO2 dispersion at different pH was shown in Figure 2(b), and the absolute value of zeta potential also increased with the increase of pH value and the dispersion can be relatively stable at pH 8.
Effect of coating process on water pressure resistance
The fabric must be waterproofed before coating to prevent the coating agent penetration. Waterproofing agent AG-E081 was used for the finishing with the pick-up of 42 per cent. The waterproof effect was evaluated and the result can reach 100 points in the water-spray test when the waterproofing agent is 10 g/L, which displayed a good waterproof effect (Table I).
Three variables were designed to explore the effect of fabric finishing process, namely, the dosage of coating adhesive; the drying temperature; and the drying time. The three-factor tri-horizontal orthogonal test was adopted.
The fabric after waterproof finishing was subjected to coating finishing, and the water-pressure resistance test was carried out. As shown in Table II, the main factor affecting the water-pressure resistance was the dosage of the coating agent. Low coating adhesive content made a thin film on the fabric surface, and easily produced defects, resulting in a decline in water-pressure. Secondly, the film-forming material was water-based PU resin and required a lower temperature. However, if the temperature was too low, the resin could not achieve the maximum cross-linking and the water-pressure resistance would also correspond to decline. In addition, adequate cross-linking of the resin required sufficient drying time.
Based on the above analysis, the optimized scheme was AIII BIII CII, and the numerical values were as follows: coating adhesive content of 60 per cent, drying temperature of 100°C, drying time of 3 min.
Effect of coating adhesive on water-pressure resistance
The waterproof finished fabrics then were coated with 40, 50, 60, 70 and 80 per cent coating adhesive for general coating finishing.
The water-pressure resistance was low with a coating adhesive content of 40 per cent (Table III), and it was because the lower solid content in the coating would cause uneven coating layer and the emergence of coating holes via water evaporation. When the content was more than 50 per cent, the value exhibited a slight increase with the solid content increased. This is because keeping the total amount of coating paste same, increasing the coating agent content will cause the coating uneven rather than improving its water-pressure resistance. When the total dosage of the coating agent was certain, increasing the content of coating adhesive will cause the coating uneven and lower water-pressure resistance. The following tests were based on 50 per cent of the coating adhesive content.
Effect of ultrafine TiO2 on anti-UV property
After waterproof finishing, nylon was finished by anti-UV coating with TiO2 content from 0 to 5 per cent and the anti-UV effect was determined.
The PU-based coating had little effect on the UV transmittance. When the dosage of TiO2 was more than 1 per cent, the UV transmittance decreased rapidly and up to AATCC 183-2014 standard for UV protection when the dosage was 3 per cent. The fabric structure of nylon was more closely, and had preferable shielding effect to long-wave UVA, leading to good UVA blocking ability and poor UVB blocking ability (Table IV).
SEM was used to characterize the uniformity of the nano-composite coating. The pristine nylon fiber without treatment had a very smooth surface [Figure 3(b)], while the surface morphology of the coated nylon fiber after being finished was not flat instead of many small holes, which may be due to evaporation of water and the results were consistent with the reason shown in Table III that the excessive increase in the amount of coating adhesive did not effectively increase the hydrostatic pressure.
Effect of nano-antimony doped tin dioxide on thermal insulation property
The thermal insulation performance of finished fabric with was evaluated by self-made insulation system. As shown in Figure 4, the heat insulation box was made of polystyrene foam. The inner cavity of the box was 26 × 18 × 15 cm, and the upper side of the box had an opening of 14 × 12 cm. The tungsten-iodine lamp was placed 50 cm above the polystyrene foam box. When testing, the fabric was placed above the opening of the box and two thermocouple thermometers were placed in the center of the underside of the cloth and the aluminum plate, respectively. Turn on the iodine tungsten lamp and recorded the temperature every 5 min until reaching the balance. The equilibrium temperature difference was used to characterize the thermal insulation properties of the finished fabric. The temperatures displayed on the two thermometers were recorded. The bottom temperature changes were shown in Figure 5(a), and the final temperature of the cloth were shown in Table V.
The insulation curves of water-soluble PU coating and the pristine nylon fabric basically coincide, which revealed that the PU coating on the fabric with no thermal insulation performance. The thermal insulation increased as the content of ATO increased, and when the content was 3 per cent, the bottom temperature reached the minimum. Continue to increase the content of ATO will make the cloth surface temperature rose instead of better thermal insulation performance, and then transferred thermal to the air inside the box, finally affected its thermal insulation property.
The temperature of the cloth surface became higher with the increase of ATO content, because of the higher thermal conductivity of ATO. Increasing the content will inevitably make the stronger absorptive capacity of thermal, resulting in heat of cloth.
To further discuss the role of nano-ATO on the light, the infrared transmittance test of the pristine fabric, PU coated fabric and fabrics with different ATO contents were tested. With the increase of ATO contents, the infrared transmittances of nylon were gradually reduced [Figure 5(b)]. According to Kirchhoff’s law of radiation, when an object is irradiated by other objects, if the absorption rate is denoted by A, R is the reflectivity and T is the transmittance, then there is: A + R + T = 1.
When the light source was applied on the coating, part of the energy was blocked (absorption and reflection) by the ATO coating, the rest penetrated through the coating into the foam box. The role of ATO was mainly on the infrared barrier attributed to the conductivity with a high concentration of free electron gas model, which possessed strong reflectivity in the low-frequency infrared region. Moreover, the doping of Sb increased the carrier concentration, resulting in the increased reflection in IR (Hu et al., 2018; Huang et al., 2015). With the dosage of ATO increased, the infrared transmittance decreased. In other words, the ability of the ATO coating to infrared blocking (A + R) increased with the increase of ATO dosage.
As shown in Table V, the cloth surface temperature increased with the amount of ATO increased, indicating that ATO had a certain absorption effect on infrared, thus, the principle of ATO insulation was the absorption and reflection of infrared (Hu et al., 2018; Li et al., 2014b).
In addition, the coating that causes itself to rise in temperature by absorbing infrared rays will continue convective heat transfer through the fabric to the box. At the same time, the foam box also dissipated heat to outside, to a certain time (about 50 min), the heat emitted was equal to the amount of heat entering the box and the system was in a state of dynamic equilibrium. The temperature in the box remained unchanged as then.
The coating absorbed infrared rays and converted heat to the inside of the box through the cloth, it also dissipated heat to the cloth surface from itself and achieved balance after 50 min, then the surface temperature no longer changed. However, the heat insulation effect did not increase with the amount of the ATO content. An increase in the ATO content increased the thermal conductivity of the cloth surface, which, in turn, aggravated the air conduction effect of the cloth to the inside of the box, causing the air temperature inside the box to rise and the cloth surface to become hot. The distribution of nano-ATO in the coating was more uniform (Figure 6) and the particles were significantly smaller than the ultrafine TiO2 coating shown in Figure 3(c).
Determination of the optimal process
To investigate the interaction relationship of nano-ATO, ultrafine TiO2 and PU coating interaction, orthogonal experiments (Table VI) were carried out and to design three variables, namely, ATO content, TiO2 content and coating content.
The nylon fabric was waterproofed according to 2.3, and then coated and finished according to the method of 2.5. The ultrafine TiO2 and nano-ATO were selected as functional materials, and applied to the fabric surface by coating, with a drying temperature of 100°C and time of 3 min. The water-pressure resistance, the property of anti-UV and the thermal insulation effect were tested and the results are shown in Table VII.
The ultrafine TiO2 was also the most important factor that affected the UV protection of nylon fabrics. All the results of the orthogonal test can meet the standards of AATCC 183-2014 “Evaluation of UV-protection properties of textiles”. From the thermal insulation effect, AIBIICII was the best combination and bottom temperature was only 52.1°C. The coating adhesive content was in the range of 50-60 per cent, and had little effect on the water impermeability. In summary, the optimal process for finishing nylon coating was AIBIICI, namely, 2 per cent of ATO, 3 per cent of TiO2 and 50 per cent of PU.
Comprehensive experiment of optimal process
According to the optimal process of nylon given in 2.6, the UV protection, thermal insulation and water pressure resistance of the nylon samples were measured (Table VIII).
The thermal insulation effect of the fabric after coating was obviously enhanced. The temperature of the box bottom decreased 8°C and the cloth surface increased 5.2°C. Meanwhile, the anti-UV performance can meet the standards of AATCC 183-2014 and the water pressure resistance was more than 10,000 Pa, fully able to meet the needs of the umbrella cloth.
The infrared transmittance, reflectance and absorbance of the pristine nylon and the finished nylon were also analyzed. It can be seen from Figure 7 that the sum of the infrared transmission, absorbance and reflectance of the fabric measured by the instrument was not equal to 1 and the absorption was relatively lower. In the infrared region (720-2,600 nm), the sum of the average of infrared transmittance, absorption and reflectance was about 90 per cent. This was because the surface of the fabric was uneven, and some of the infrared rays were scattered by the fabric and cannot be tested by the instrument. After coating, the sum of the three average values was less than 50 per cent, while the transmittance had dropped significantly. This was because of the addition of nano-materials, which increased the surface roughness of the, lead to an increase in the scattering of light and blocks the transmission of light.
The thermal insulation mechanism of ultrafine TiO2 and nano-ATO may be the absorption and scattering of sunlight by the powder, which prevent sunlight from passing through the fabric, thereby reducing the temperature under the cloth.
In addition, the thermal insulation performance of the fabric coated by the optimal process was also tested using an open system [Figure 8(a)].
As can be seen from Figure 8(b), in the open system test, the nano-coated fabric can still guarantee a certain thermal insulation effect and the temperature of the aluminum plate was about 3°C lower than that of the unfinished fabric.
The ultrafine TiO2 and nano-ATO were used as the UV protective and thermal insulated powders, and were dispersed in the water through the ball milling and ultrasonic method. The ultrafine TiO2 and nano-ATO can be stably dispersed in the water by the action of sodium polycarboxylate at pH 8-9. Before functional coatings, the nylon fabric was water-repellent finished and had a waterproof score of 100. After finishing by the optimal process, the UPF was more than 50, UVA was less than 5 per cent, which meet the standards to AATCC 183-2014 “Evaluation of UV-protection property of textiles”; in the thermal insulation performance test, it can reduce the temperature by 8-9°C using the self-made closed system and decrease by about 3°C using the open system temperature; pressure resistance was more than 10,000 Pa, to meet the requirements of the umbrella cloth waterproof performance.
The UV-proof performance of fabrics after functional coatings meets national standards and the water pressure resistance also meets the needs of general umbrellas and tarpaulins. The role of ATO is mainly the absorption and reflection of infrared rays; the incorporation of TiO2 effectively shields not only the UV but also some of the visible light and infrared rays. The outdoor fabric developed by this method can effectively block UV and solar radiation, and adopts an environmentally-friendly water-based PU coating to reduce environmental pollution.
Orthogonal experimental design of coating process
|A: dosage (Wt. %)||40||50||60|
|B: drying temperature (T/°C)||60||80||100|
|C: drying time (t/min)||1||3||5|
Orthogonal experimental results of coating process
Effect of coating agent content on water-pressure resistance
|Coating adhesive content (%)||40||50||60||70||80|
Anti-UV effect of ultrafine TiO2 finished nylon
Effect of ATO content on the cloth surface equilibrium temperature
Orthogonal design of optimal process
|C Coating adhesive/%||50||55||60|
Orthogonal test analysis of fabric after functional coating
|Item||A||B||C||UPF||UVA (%)||Bottom temperature
|UPF analysis||UVA analysis|
|Temperature analysis||Waterproof analysis|
The performance of the fabric after finishing with the optimal process
|Item||UPF||UVA (%)||Bottom temperature/°C||Cloth temperature/°C||Waterproof/
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This study was fund by Funding of Hebei Education Department（Grant No.QN2018038）and excellent Youth Talents Plan of Hebei Province. The authors wish to thank the academic team of Textile Cleaner Production and Functional Advanced Processing Technology” for the support during this research.